Author
Topic: Safrole isomerization under vacuum (Read 1633 times)

bbeeasheets

ok, i just purchased a sargent-welch 1405 duo seal vacuum pump. unbelievably to me, it distills safrole at 64C! (100 degrees lower than my last pump) my question is, i prefer to isomerize under vacuum (i heat to just boiling, but where it doesn't distill), and when boiling ceases the isomerization is complete. Will safrole isomerize (with KOH) at 60C?

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Rhodium

At 60°C the isomerization will take days, if it at all will go to completion. Use another pump or use a bleed valve with this one (something as low-tech as a leaky rubber tube is fine, adjust the vacuum by pricking holes into it with a pin).

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ApprenticeCook

all the vacuum is required for here is to remove excess water as this is a killer, but rhodium is right i use my aspirator... or just put deliberate leaks in the system you have.... but thats a nice pump for disto, good on ya!

Hey just a question from me....Is there some relationship table/grpah around that has the isomerisation rxn times vs temp??? just so i know what the ideal temp for the rxn to be is to achieve the better yields....